Unsaturated silanol composition and application thereof in skin care
By using unsaturated silanol compositions, plant essential oil microcapsules were prepared using modified agar and modified β-cyclodextrin. Combined with organosilanol stabilizers, this solved the problem of poor moisturizing longevity in skincare products, achieved skin barrier repair and highly effective antibacterial and antiseptic effects, and improved the overall skincare efficacy of the products.
Patent Information
- Application Number
- CN202511559872.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-10-29
- Publication Date
- 2025-12-23
AI Technical Summary
Existing skincare products have a single moisturizing mechanism, which cannot achieve comprehensive protection, has poor moisturizing effect, and weak transdermal penetration, thus failing to meet market demand.
An unsaturated silanol composition is used, comprising organosilanol, plant essential oil microcapsules, glycerin, hyaluronic acid, and caprylic/capric acid polyethylene glycol glyceride. Plant essential oil microcapsules are prepared by compounding modified agar and modified β-cyclodextrin with sodium alginate, and combined with organosilanol stabilizers to achieve moisturizing, anti-aging, barrier repair, and antibacterial and preservative effects.
It significantly improves the stability and lifespan of skincare products, enhances moisturizing and water-locking effects, extends the lifespan of products, and possesses excellent skin barrier repair and highly effective antibacterial and preservative capabilities.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of skincare technology, specifically relating to a composition of unsaturated silanol and its application in skincare. Background Technology
[0002] Silanols, as organosilicon compounds, are characterized by containing at least one silanol functional group. They can be understood as the active form of silicon in living organisms. The difference between them and inorganic silicon is that the abundant silicon in the Earth's crust (existing in the form of silicon dioxide and silicates) is inorganic and difficult for the human body to directly absorb and utilize. Silanols, on the other hand, are organosilicon with extremely high bioavailability and can be effectively utilized by human cells. The difference between them and silicone is that common silicone is an inert high-molecular-weight polymer used in skincare products for filling and lubrication, and cannot be absorbed by the skin or participate in biological processes. Silanols, however, are small molecules with biological activity and can be directly absorbed by the skin and enter cells without complex metabolic transformations.
[0003] With the improvement of living standards, people are paying more and more attention to skin care and have higher requirements for the efficacy of skin care products. As an important reservoir of water in the human body, the skin stores 18-20% of the body's total water content. Its water content is closely related to the health of the skin; therefore, "moisturizing" is a perennial theme in skin care products. If the skin is dehydrated, it will lead to epidermal barrier dysfunction, causing various skin problems (such as dryness, spots, acne, pimples, sensitivity, enlarged pores, dullness, wrinkles, and sagging), and even various skin diseases. Currently, skin care products with moisturizing effects on the market have a single moisturizing mechanism and cannot achieve comprehensive protection. Furthermore, simple moisturizing is no longer sufficient to meet market demands, exhibiting shortcomings such as poor moisturizing duration, weak transdermal absorption, and limited functionality. Summary of the Invention
[0004] To address the shortcomings mentioned in the background art, the present invention aims to provide a composition of unsaturated silanols and its application in skincare, thereby preparing a composition of unsaturated silanols with good skin barrier repair and moisturizing effects, while also possessing highly efficient and long-lasting antibacterial and preservative capabilities.
[0005] The objective of this invention can be achieved through the following technical solutions: A composition of unsaturated silanols, comprising the following raw materials in parts by weight: 5-30 parts of organosilanols, 1-5 parts of plant essential oil microcapsules, 2-7 parts of glycerin, 0.2-0.5 parts of hyaluronic acid, 1-3 parts of caprylic / capric acid polyethylene glycol glyceride, and 15-60 parts of purified water; The organosilasanol has the general formula X-Si(OH)2-Y; wherein: group X is vinyl, allyl, straight-chain or branched C1~C4 alkyl group; group Y is vinyl, allyl, -OCH3, -OCH2CH3, -OCH2OH, -OCH2CH2OH, straight-chain or branched C1~C4 alkyl group; The method for preparing the organosilanol includes the following steps: adding an organosilanol stabilizer to purified water, then adding a diol solvent, and under argon protection, slowly adding allyl trichlorosilane, adjusting the pH to neutral, to prepare the organosilanol; The plant essential oil microcapsules are made by using modified agar, modified β-cyclodextrin and sodium alginate as wall materials, plant essential oil as core material and calcium chloride as crosslinking agent, through extrusion and freeze-drying methods; the modified agar is made by esterification reaction of octenyl succinic anhydride and agar; the modified β-cyclodextrin is made by reacting β-cyclodextrin with p-toluenesulfonyl chloride, and then grafting the prepared mono-6-p-toluenesulfonyl-β-cyclodextrin with chitosan.
[0006] Preferably, the organosilanol stabilizer is one or a combination of several of dihydroaerol alkaloids, resveratrol oxide, mannulic acid, gallic acid, conopeptide, and acetyl hexapeptide-8; and the diol solvent is one or a combination of several of propylene glycol, butanediol, methylpropylene glycol, pentanediol, and hexanediol.
[0007] Preferably, the method for preparing the plant essential oil microcapsules includes the following steps: I. Dissolve modified β-cyclodextrin in acetic acid solution to obtain solution one. Dissolve sodium alginate and modified agar in purified water by ultrasonication at 45°C to form homogeneous solution two. II. Use 1% Tween 80 emulsified plant essential oils were mixed with solution two for 2-3 hours to obtain solution three. III. Take solution one and add calcium chloride solution to carry out cross-linking reaction, then adjust the pH value to 5.1~5.4 with sodium hydroxide solution, stir and mix at room temperature to obtain solution four; IV. Using a syringe, solution three is dripped at a constant rate into solution four while it is being stirred to form a microcapsule suspension. The microcapsules are then solidified at 4°C. Subsequently, they are repeatedly washed with purified water to remove surface impurities. After filtration and freeze-drying, plant essential oil microcapsules are prepared.
[0008] Preferably, the ratio of modified β-cyclodextrin, sodium alginate, and modified agar wall material is 1~4:1:1; the ratio of core material plant essential oil to wall material is 1:2~3.
[0009] Preferably, the calcium chloride solution has a mass concentration of 1-3%; the plant essential oil is one or more of the following: citrus essential oil, rose essential oil, thyme essential oil, peppermint essential oil, lemon essential oil, chamomile essential oil, and lavender essential oil.
[0010] Preferably, the preparation method of modified β-cyclodextrin in step I includes the following steps: ① Take β-cyclodextrin, purified water and sodium hydroxide solution in a reactor, place in an ice bath, and after the solution becomes clear, slowly add p-toluenesulfonyl chloride dissolved in acetonitrile. Stir the reaction under ice bath conditions for 2-3 hours, then adjust the pH value to 5.5-6 with hydrochloric acid solution, place at 4℃ overnight, then filter under reduced pressure, recrystallize the precipitate and dry it to prepare mono-6-p-toluenesulfonyl-β-cyclodextrin; ② Chitosan was dissolved in glacial acetic acid to prepare a chitosan solution. Mono-6-p-toluenesulfonyl-β-cyclodextrin was dissolved in N,N-dimethylformamide and added to the chitosan solution. The mixture was stirred at 95~100℃ for 20~24h, then cooled to room temperature. The pH of the system was adjusted to neutral using sodium hydroxide and left at 4℃ overnight. The mixture was then transferred to a dialysis bag and immersed in 100 times its volume of purified water for dialyzing. Finally, the mixture was freeze-dried under vacuum to obtain modified β-cyclodextrin.
[0011] Preferably, the sodium hydroxide solution has a mass concentration of 0.3~0.35 g / mL; the addition ratio of β-cyclodextrin, purified water, sodium hydroxide solution and p-toluenesulfonyl chloride is 2.5~4 g: 20~30 mL: 0.5~1.5 mL: 0.4~0.6 g; and the mass ratio of chitosan and mono-6-p-toluenesulfonyl-β-cyclodextrin is 1:2.5~4.
[0012] Preferably, the preparation method of modified agar in step I includes the following steps: dissolving agar powder in purified water to prepare an agar solution and adjusting the pH value to 8-8.5 using sodium hydroxide, then adding a mixed solution of isopropanol and octenyl succinic anhydride dropwise, maintaining the pH value at 8-8.5 during the reaction, reacting at 35-40℃ for 2-3 hours, and then adjusting the pH value of the system to 6.5 with hydrochloric acid solution to terminate the reaction, followed by filtration, washing, and drying to obtain modified agar.
[0013] Preferably, the addition ratio of agar powder, purified water, isopropanol and octenyl succinic anhydride is 2.5~7.5g:100mL:8~12mL:2~3mL.
[0014] The application of the unsaturated silanol composition as described above in skincare involves mixing parts by weight of the raw materials to prepare the unsaturated silanol composition for use in lotions, gels, or creams.
[0015] The beneficial effects of this invention are: This invention utilizes the esterification reaction between octenyl succinic anhydride and agar to introduce hydrophobic hydrocarbon chains into the hydrophilic structure of agar, thus preparing a modified agar with amphiphilic properties. The modified agar, modified β-cyclodextrin, and sodium alginate are combined as a wall material, plant essential oils as the core material, and calcium chloride as a crosslinking agent. Plant essential oil microcapsules are prepared by extrusion and freeze-drying methods, avoiding the loss of plant essential oils caused by high temperature and high pressure. Simultaneously, it effectively prevents adverse reactions such as oxidation, photolysis, and pyrolysis of the active ingredients in plant essential oils, significantly improving the stability of skincare products. Furthermore, the microcapsules enable the slow and continuous release of active ingredients from plant essential oils, helping to enhance the durability of skincare effects, extend the product's usage cycle, and improve the consumer experience.
[0016] This invention utilizes a two-step method to prepare chitosan-grafted modified β-cyclodextrin. Chitosan exhibits excellent skin retention and penetration, as well as antibacterial and moisturizing effects. Its positive charge can combine with the negative charge on the skin surface, thereby adhering to the skin surface and increasing the local concentration of active ingredients. β-cyclodextrin possesses good biocompatibility and is non-toxic and non-irritating. Its structural unit contains both a hydrophilic shell and a hydrophobic cavity. The hydrophobic cavity can encapsulate plant essential oils to form inclusion complexes. The hydrophilic modification groups improve the water solubility of the chitosan bound to it, thereby increasing the stability and bioavailability of plant essential oils. It also has a good sustained-release effect, which can promote the transdermal penetration of active ingredients in plant essential oils.
[0017] This invention utilizes organosilanol stabilizers, glycol solvents, allyltrichlorosilane, and purified water to prepare organosilanols. This allows the composition to possess the anti-inflammatory and anti-allergic effects of the bioactive organosilanol stabilizer, while also exhibiting the moisturizing, anti-aging, and barrier-repairing effects of unsaturated silanols. The organosilanol stabilizer is a bioactive substance, ensuring the prepared composition provides moisturizing, antioxidant, and barrier-repairing effects. The plant essential oil microcapsules contain chitosan and the antibacterial activity of plant essential oils, thus exerting a good antibacterial effect. When applied to skincare products, they achieve a preservative effect. Simultaneously, microcapsule technology can delay the release of plant essential oils, isolate them from the external environment, protect their activity and improve their stability, reduce the irritation of the plant essential oil microcapsules, and promote transdermal penetration. Detailed Implementation
[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0019] Example 1 A method for preparing organosilanol includes the following steps: 50g of organosilanol stabilizer dihydrooat alkaloid is added to 800mL of purified water, followed by 200mL of diol solvent methyl propylene glycol. Under argon protection, 30g of allyl trichlorosilane is slowly added dropwise, and the pH is adjusted to neutral to obtain a colorless, clear, and transparent solution of organosilanol.
[0020] Example 2 A method for preparing modified β-cyclodextrin includes the following steps: ① Take 30g of β-cyclodextrin, 250mL of purified water and 10mL of sodium hydroxide solution with a mass concentration of 0.34g / mL in a reactor, place it in an ice bath, and after the solution becomes clear, slowly add 5g of p-toluenesulfonyl chloride dissolved in 15mL of acetonitrile. Stir the reaction for 2h under ice bath conditions, then adjust the pH to 6 with 10% hydrochloric acid solution, place it at 4℃ overnight, and then filter under reduced pressure. The precipitate is recrystallized with purified water at 85℃ and dried to prepare mono-6-p-toluenesulfonyl-β-cyclodextrin. ② Dissolve 1g of chitosan in 80mL of 1% glacial acetic acid to prepare a chitosan solution. Dissolve 3g of mono-6-p-toluenesulfonyl-β-cyclodextrin in 40mL of N,N-dimethylformamide and add it to the chitosan solution. Stir and react at 100℃ for 24h. Then cool to room temperature, adjust the pH of the system to neutral using sodium hydroxide, and place at 4℃ overnight. Then transfer to a dialysis bag (MW12000) and immerse in 100 times the volume of purified water for dialyzing. Finally, freeze dry under vacuum to prepare modified β-cyclodextrin.
[0021] Example 3 A method for preparing modified agar includes the following steps: dissolving 5g of agar powder in 100mL of purified water to prepare an agar solution and adjusting the pH to 8.5 using sodium hydroxide. Then, adding a mixed solution of 10mL isopropanol and 2.5mL octenyl succinic anhydride dropwise, maintaining the pH at 8.5 during the reaction, reacting at 40℃ for 2 hours, and then adjusting the pH to 6.5 with 1mol / L hydrochloric acid solution to terminate the reaction. Subsequently, the modified agar is obtained by filtration, washing, and drying.
[0022] Example 4 A method for preparing plant essential oil microcapsules includes the following steps: I. Dissolve the modified β-cyclodextrin prepared in Example 1 in 1% acetic acid solution to prepare a solution with a mass percentage concentration of 0.57 wt%. Dissolve sodium alginate and modified agar prepared in Example 2 in purified water at a mass ratio of 1:1 at 45°C to prepare a homogeneous solution with a mass percentage concentration of 2 wt%. The wall material ratio of modified β-cyclodextrin, sodium alginate and modified agar is 3:1:1. II. Use 1% Tween 80 emulsified rose essential oil was mixed with solution two for 3 hours. The ratio of rose essential oil to wall material was 1:3, resulting in solution three. III. Take solution one and add 1.5g of calcium chloride solution with a mass concentration of 2% to carry out the cross-linking reaction. Then, adjust the pH value to 5.2 with 10% sodium hydroxide solution and stir and mix at room temperature to obtain solution four. IV. Using a syringe, solution three is dripped at a constant rate into solution four while it is being stirred to form a microcapsule suspension. The microcapsules are then solidified at 4°C. Subsequently, they are repeatedly washed with purified water to remove surface impurities. After filtration and freeze-drying, plant essential oil microcapsules are prepared.
[0023] Example 5 A composition of unsaturated silanols comprising the following components in parts by weight: 5.5 parts of organosilanol prepared in Example 1, 1.2 parts of plant essential oil microcapsules prepared in Example 4, 2.3 parts of glycerin, 0.25 parts of hyaluronic acid, 1.4 parts of polyethylene glycol glyceride caprylate and caprylic acid, and 18 parts of purified water.
[0024] The preparation method of the above-mentioned unsaturated silanol composition includes the following steps: weighing each raw material according to the weight parts, and mixing the raw materials according to the weight parts to prepare the unsaturated silanol composition.
[0025] Example 6 A composition of unsaturated silanols comprising the following components in parts by weight: 17 parts of organosilanol prepared in Example 1, 3 parts of plant essential oil microcapsules prepared in Example 4, 4.1 parts of glycerin, 0.33 parts of hyaluronic acid, 2.2 parts of polyethylene glycol glyceride caprylate and capric acid, and 41 parts of purified water.
[0026] The preparation method of the above-mentioned unsaturated silanol composition is the same as that in Example 5.
[0027] Example 7 A composition of unsaturated silanols comprising the following components in parts by weight: 28 parts of organosilanol prepared in Example 1, 4.8 parts of plant essential oil microcapsules prepared in Example 4, 6.3 parts of glycerin, 0.44 parts of hyaluronic acid, 2.6 parts of polyethylene glycol glyceride caprylate and caprylic acid, and 55 parts of purified water.
[0028] The preparation method of the above-mentioned unsaturated silanol composition is the same as that in Example 5.
[0029] Comparative Example 1 A method for preparing plant essential oil microcapsules includes the following steps: I. Dissolve β-cyclodextrin in 1% acetic acid solution to prepare a solution with a mass percentage concentration of 0.57 wt%. Dissolve sodium alginate and modified agar prepared in Example 2 in purified water at a mass ratio of 1:1 at 45°C to prepare a homogeneous solution with a mass percentage concentration of 2 wt%. The wall material ratio of β-cyclodextrin, sodium alginate and modified agar is 3:1:1. II. Use 1% Tween 80 emulsified rose essential oil was mixed with solution two for 3 hours. The ratio of rose essential oil to wall material was 1:3, resulting in solution three. III. Take solution one and add 1.5g of calcium chloride solution with a mass concentration of 2% to carry out the cross-linking reaction. Then, adjust the pH value to 5.2 with 10% sodium hydroxide solution and stir and mix at room temperature to obtain solution four. IV. Using a syringe, solution three is dripped at a constant rate into solution four while it is being stirred to form a microcapsule suspension. The microcapsules are then solidified at 4°C. Subsequently, they are repeatedly washed with purified water to remove surface impurities. After filtration and freeze-drying, plant essential oil microcapsules are prepared.
[0030] Comparative Example 2 A method for preparing plant essential oil microcapsules includes the following steps: I. Dissolve the modified β-cyclodextrin prepared in Example 1 in 1% acetic acid solution to prepare a solution with a mass percentage concentration of 0.57wt%. Dissolve sodium alginate and agar in purified water at a mass ratio of 1:1 at 45°C to prepare a homogeneous solution with a mass percentage concentration of 2wt%. The wall material ratio of modified β-cyclodextrin, sodium alginate and agar is 3:1:1. II. Use 1% Tween 80 emulsified rose essential oil was mixed with solution two for 3 hours. The ratio of rose essential oil to wall material was 1:3, resulting in solution three. III. Take solution one and add 1.5g of calcium chloride solution with a mass concentration of 2% to carry out the cross-linking reaction. Then, adjust the pH value to 5.2 with 10% sodium hydroxide solution and stir and mix at room temperature to obtain solution four. IV. Using a syringe, solution three is dripped at a constant rate into solution four while it is being stirred to form a microcapsule suspension. The microcapsules are then solidified at 4°C. Subsequently, they are repeatedly washed with purified water to remove surface impurities. After filtration and freeze-drying, plant essential oil microcapsules are prepared.
[0031] Comparative Example 3 A composition of unsaturated silanols comprising the following components in parts by weight: 28 parts of organosilanol prepared in Example 1, 4.8 parts of plant essential oil microcapsules prepared in Comparative Example 1, 6.3 parts of glycerin, 0.44 parts of hyaluronic acid, 2.6 parts of polyethylene glycol glyceride caprylate and capric acid, and 55 parts of purified water.
[0032] The preparation method of the above-mentioned unsaturated silanol composition is the same as that in Example 5.
[0033] Comparative Example 4 A composition of unsaturated silanols comprising the following components in parts by weight: 28 parts of organosilanol prepared in Example 1, 4.8 parts of plant essential oil microcapsules prepared in Comparative Example 2, 6.3 parts of glycerin, 0.44 parts of hyaluronic acid, 2.6 parts of polyethylene glycol glyceride caprylate and capric acid, and 55 parts of purified water.
[0034] The preparation method of the above-mentioned unsaturated silanol composition is the same as that in Example 5.
[0035] Comparative Example 5 A composition of unsaturated silanols comprising the following components in parts by weight: 28 parts of organosilanol prepared in Example 1, 4.8 parts of rose essential oil, 6.3 parts of glycerin, 0.44 parts of hyaluronic acid, 2.6 parts of octanoic acid-capric acid-polyethylene glycol glyceride, and 55 parts of purified water.
[0036] The preparation method of the above-mentioned unsaturated silanol composition is the same as that in Example 5.
[0037] Comparative Example 6 A composition of unsaturated silanols comprising the following components in parts by weight: 4.8 parts of plant essential oil microcapsules prepared in Example 4, 6.3 parts of glycerin, 0.44 parts of hyaluronic acid, 2.6 parts of octanoic acid-capric acid-polyethylene glycol glyceride, and 55 parts of purified water.
[0038] The preparation method of the above-mentioned unsaturated silanol composition is the same as that in Example 5.
[0039] Performance testing The compositions of unsaturated silanols prepared in Examples 5-7 and Comparative Examples 3-6 were subjected to performance testing: (1) Skin irritation test: 32 subjects were selected. 1 mL of the prepared composition was applied to the test chamber of the spot tester and then applied to the back or flexor side of the forearm of the subject with special adhesive tape. After 24 hours, the spot tester was removed. If there was any remaining product, it was gently wiped away with a damp tissue. Skin reactions were observed at 0.5 hours, 24 hours, and 48 hours, and the results were recorded according to the skin reaction grading criteria in Table 1. Table 1. Skin Reaction Grading Standards In the closed patch test, 32 subjects showed no adverse reactions after using the unsaturated silanol composition for 0.5h, 24h and 48h. No symptoms such as erythema, burning sensation or itching were observed. The results were negative, indicating that the prepared unsaturated silanol composition is non-irritating to the skin.
[0040] (2) Antibacterial performance test: Take 30 mL of the prepared composition into a sterilized conical flask, and inoculate with 0.3 mL of a mixture with a concentration of 1×10⁻⁶. 6 A mixed bacterial suspension of S. aureus, E. coli, and P. aeruginosa (CFU / mL) was vortexed until homogeneous and allowed to stand. The samples were then stored in a dry, well-ventilated place at room temperature (20°C–25°C). Colony counts were tested every 7 days for 28 days after inoculation. 1 mL of sample was transferred and logarithmically diluted with sterile physiological saline to an appropriate concentration. The microbial content was calculated using the plate count method. Each group was tested in triplicate. Evaluation criteria were referenced from the Personal Care Products Council. ① When the bacteria count is <10 CFU / mL starting from day 7, it indicates that the system has excellent antibacterial properties and passes the challenge test, thus being rated as Grade A; ② On day 28, when the bacterial count was between 10 and 100 CFU / mL, it indicated that the system had good antibacterial properties and passed the challenge test, thus being rated as Grade B. ③ If the bacteria count is between 100 and 1000 CFU / mL on day 28, it indicates that the antibacterial performance of the system is average. It can pass the challenge test under certain conditions and be rated as grade C. ④ On day 28, if the bacteria count is >1000 CFU / mL, it indicates that the antibacterial performance of the system is relatively poor. It is considered to fail the challenge test and is rated as grade D. The data results are shown in Table 2.
[0041] Table 2 Results of Antibacterial Performance Tests on Samples As can be seen from the data in Table 2, the compositions prepared in Examples 5-7 of this invention have very efficient and long-lasting antibacterial capabilities. Among them, the plant essential oil microcapsules added in Comparative Example 3 did not modify β-cyclodextrin, and rose essential oil was directly added in Comparative Example 5. The antibacterial levels in Comparative Examples 3 and 5 were lower than those in Examples 5-7, indicating that the preparation of modified β-cyclodextrin and plant essential oil microcapsules improved the sustained-release effect of the composition to a certain extent, and the long-lasting antibacterial ability was excellent.
[0042] (3) Moisturizing function and skin barrier function test: 56 subjects with an average age of 25-45 years were selected, including 28 females and 28 males, and randomly divided into 7 groups of 8 subjects each. The subjects had healthy skin and met the inclusion criteria. The test was conducted at a room temperature of 20℃ and a relative humidity of 35% for at least half an hour. A 5cm×5cm test area was drawn on the inner side of the subject's right forearm. The skin in the test area was peeled off with tape 10 times and then the test sample was applied. The sample volume was 1mL. The moisturizing function and skin barrier function were tested. ① Moisturizing function test: Using a Corneometer CM825, the skin moisture content was tested before, after, and 4 hours after the sample was applied. Each test was repeated three times, and the average value was calculated. The skin moisture content growth rate was calculated using the following formula: Skin moisture content growth rate = (M1-M2) / M2×100%, where M2 is the skin moisture content before application and M1 is the skin moisture content after application. The data results are shown in Table 3. ② Skin Barrier Function Test: Using the Tewameter TM300, the amount of skin moisture loss was tested before, after, and 6 hours after the sample was applied. Each test was repeated three times, and the average value was calculated. The rate of change of the TEWL value was calculated. The TEWL value is an important parameter describing the skin barrier and is closely related to the water content of the stratum corneum. The higher the TEWL value, the more water is lost through the skin and the poorer the barrier function of the stratum corneum. The data results are shown in Table 3.
[0043] Table 3. Results of the tests on the moisturizing function and skin barrier function of the samples. As can be seen from the data in Table 3, the compositions prepared in Examples 5-7 of this invention possess good skin barrier repair and moisturizing / water-locking effects. Specifically, the plant essential oil microcapsules added in Comparative Example 3 did not modify β-cyclodextrin, the plant essential oil microcapsules added in Comparative Example 4 did not modify agar, rose essential oil was directly added in Comparative Example 5, and no organosilanols were added in Comparative Example 6. The measured growth rate of water content in Comparative Examples 3-6 was lower than that in Examples 5-7, and the transdermal water loss was more significant than in Examples 5-7. This indicates that the introduction of plant essential oil microcapsules and organosilanols can prolong the moisturizing / water-locking effect of the compositions and reduce transdermal water loss.
[0044] In the description of this specification, references to terms such as "an embodiment," "example," "specific example," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the invention. In this specification, illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples.
[0045] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention.
Claims
1. A composition of unsaturated silanols, characterized in that, The ingredients include the following parts by weight: 5-30 parts organosilanol, 1-5 parts plant essential oil microcapsules, 2-7 parts glycerin, 0.2-0.5 parts hyaluronic acid, 1-3 parts caprylic / capric acid polyethylene glycol glyceride, and 15-60 parts purified water; The organosilasanol has the general formula X-Si(OH)2-Y; wherein: group X is vinyl, allyl, straight-chain or branched C1~C4 alkyl group; group Y is vinyl, allyl, -OCH3, -OCH2CH3, -OCH2OH, -OCH2CH2OH, straight-chain or branched C1~C4 alkyl group; The method for preparing the organosilanol includes the following steps: adding an organosilanol stabilizer to purified water, then adding a diol solvent, and under argon protection, slowly adding allyl trichlorosilane, adjusting the pH to neutral, to prepare the organosilanol; The plant essential oil microcapsules are made by using modified agar, modified β-cyclodextrin and sodium alginate as wall materials, plant essential oil as core material and calcium chloride as crosslinking agent, through extrusion and freeze-drying methods; the modified agar is made by esterification reaction of octenyl succinic anhydride and agar; the modified β-cyclodextrin is made by reacting β-cyclodextrin with p-toluenesulfonyl chloride, and then grafting the prepared mono-6-p-toluenesulfonyl-β-cyclodextrin with chitosan.
2. The composition of unsaturated silanols according to claim 1, characterized in that, The organosilanol stabilizer is one or a combination of several of the following: dihydroaerol, resveratrol oxide, mannouric acid, gallic acid, conopeptide, and acetyl hexapeptide-8; the diol solvent is one or a combination of several of the following: propylene glycol, butanediol, methylpropylene glycol, pentanediol, and hexanediol.
3. The composition of unsaturated silanols according to claim 1, characterized in that, The preparation method of the plant essential oil microcapsules includes the following steps: I. Dissolve modified β-cyclodextrin in acetic acid solution to obtain solution one. Dissolve sodium alginate and modified agar in purified water by ultrasonication at 45°C to form homogeneous solution two. II. Use 1% Tween 80 emulsified plant essential oils were mixed with solution two for 2-3 hours to obtain solution three. III. Take solution one and add calcium chloride solution to carry out cross-linking reaction, then adjust the pH value to 5.1~5.4 with sodium hydroxide solution, stir and mix at room temperature to obtain solution four; IV. Using a syringe, solution three is dripped at a constant rate into solution four while it is being stirred to form a microcapsule suspension. The microcapsules are then solidified at 4°C. Subsequently, they are repeatedly washed with purified water to remove surface impurities. After filtration and freeze-drying, plant essential oil microcapsules are prepared.
4. The composition of unsaturated silanols according to claim 3, characterized in that, The ratio of modified β-cyclodextrin, sodium alginate, and modified agar wall material is 1~4:1:1; the ratio of core material plant essential oil to wall material is 1:2~3.
5. The composition of unsaturated silanols according to claim 3, characterized in that, The calcium chloride solution has a mass concentration of 1-3%; the plant essential oil is one or more of the following: citrus essential oil, rose essential oil, thyme essential oil, peppermint essential oil, lemon essential oil, chamomile essential oil, and lavender essential oil.
6. The composition of unsaturated silanols according to claim 3, characterized in that, The preparation method of modified β-cyclodextrin in step I includes the following steps: ① Take β-cyclodextrin, purified water and sodium hydroxide solution in a reactor, place in an ice bath, and after the solution becomes clear, slowly add p-toluenesulfonyl chloride dissolved in acetonitrile. Stir the reaction under ice bath conditions for 2-3 hours, then adjust the pH value to 5.5-6 with hydrochloric acid solution, place at 4℃ overnight, then filter under reduced pressure, recrystallize the precipitate and dry it to prepare mono-6-p-toluenesulfonyl-β-cyclodextrin; ② Chitosan was dissolved in glacial acetic acid to prepare a chitosan solution. Mono-6-p-toluenesulfonyl-β-cyclodextrin was dissolved in N,N-dimethylformamide and added to the chitosan solution. The mixture was stirred at 95~100℃ for 20~24h, then cooled to room temperature. The pH of the system was adjusted to neutral using sodium hydroxide and left at 4℃ overnight. The mixture was then transferred to a dialysis bag and immersed in 100 times its volume of purified water for dialyzing. Finally, the mixture was freeze-dried under vacuum to obtain modified β-cyclodextrin.
7. The composition of unsaturated silanols according to claim 6, characterized in that, The sodium hydroxide solution has a mass concentration of 0.3~0.35 g / mL; the addition ratio of β-cyclodextrin, purified water, sodium hydroxide solution and p-toluenesulfonyl chloride is 2.5~4 g: 20~30 mL: 0.5~1.5 mL: 0.4~0.6 g; the mass ratio of chitosan and mono-6-p-toluenesulfonyl-β-cyclodextrin is 1:2.5~4.
8. The composition of unsaturated silanols according to claim 3, characterized in that, The preparation method of modified agar in step I includes the following steps: dissolving agar powder in purified water to prepare an agar solution and adjusting the pH value to 8-8.5 using sodium hydroxide. Then, adding a mixed solution of isopropanol and octenyl succinic anhydride dropwise, maintaining the pH value at 8-8.5 during the reaction, reacting at 35-40℃ for 2-3 hours, and then adjusting the pH value of the system to 6.5 with hydrochloric acid solution to terminate the reaction. Subsequently, the modified agar is prepared by filtration, washing, and drying.
9. The composition of unsaturated silanols according to claim 8, characterized in that, The addition ratio of agar powder, purified water, isopropanol and octenyl succinic anhydride is 2.5~7.5g:100mL:8~12mL:2~3mL.
10. The application of a composition of unsaturated silanol as described in claim 1 in skin care, characterized in that, Compositions prepared by mixing parts by weight of raw materials to prepare unsaturated silanols are applied to emulsions, gels, or creams.
